CN112198130A - Method for rapidly detecting antibacterial performance of antibacterial ABS product in production - Google Patents

Method for rapidly detecting antibacterial performance of antibacterial ABS product in production Download PDF

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CN112198130A
CN112198130A CN202011138191.XA CN202011138191A CN112198130A CN 112198130 A CN112198130 A CN 112198130A CN 202011138191 A CN202011138191 A CN 202011138191A CN 112198130 A CN112198130 A CN 112198130A
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antibacterial
abs
content
metal
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郝春波
王月
刘万胜
王岩
赵欣麟
武天希
孙鹤宇
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North Huajin Chemical Industries Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/3103Atomic absorption analysis
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/223Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416Systems
    • G01N27/48Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N2021/3196Correlating located peaks in spectrum with reference data, e.g. fingerprint data

Abstract

The invention discloses a method for rapidly detecting antibacterial performance of an antibacterial ABS product in production. Placing quantitative antibacterial ABS plastic particles into a quartz crucible, performing full ashing in a high-temperature furnace, performing acidolysis dissolution, drying, dissolution to constant volume, dilution acidification, interference prevention and other treatment on ash substances cooled to room temperature by using an acid solution, an alkali solution or water, measuring the concentration of metal ions in the solution, and calculating the content of targeted metal in the antibacterial ABS plastic particles; and (4) determining the antibacterial performance of the antibacterial ABS by combining the effective antibacterial concentration of the antibacterial agent. According to the invention, the concentration of the target metal ions is measured, the content of the target metal in the antibacterial ABS plastic particles is calculated, the antibacterial effect of the antibacterial ABS is judged by combining the effective antibacterial concentration of the antibacterial agent, the problems that the antibacterial effect period of the antibacterial ABS is long and the production cannot be guided in time due to microbiological detection can be solved, and the qualification rate, the continuous operation period and the yield of products can be effectively improved.

Description

Method for rapidly detecting antibacterial performance of antibacterial ABS product in production
Technical Field
The invention relates to the technical field of antibacterial ABS production, in particular to a detection method which can quickly and accurately judge the antibacterial property of ABS by detecting the targeted metal content of an antibacterial agent in ABS plastic and combining the targeted metal content with an antibacterial effect standard curve in the antibacterial ABS production.
Background
Microorganisms are distributed in the air, soil and water in nature and are closely related to people. On one hand, the rotten dead bodies and fallen leaves can be decomposed, and the environment is purified; on the other hand, agricultural and sideline products are corroded to deteriorate, production is damaged, particularly, pathogenic microorganisms can rapidly spread disease sources, and the harm to the health of people and livestock is great. With the improvement of living standard of people, the requirement of improving the living environment of human beings is more and more urgent, and the inhibition of the growth of harmful microorganisms is an important link. Since the eighties, developed countries represented by japan began to apply antibacterial and mildewproof materials to household appliances, chemical building materials, telecommunication products, food packaging, daily necessities, bath equipment, toys, and the like, and the application of polymer materials represented by antibacterial plastics has a very important meaning for reducing the spread of diseases and the pollution to the environment.
The inhibition of the growth of microorganisms in medical microbiology mainly adopts physical and chemical methods, and can be classified into sterilization, disinfection (disinfection), bacteriostasis or antisepsis and the like according to different inhibition degrees, and the meanings are different.
And (3) sterilization: a method or effect capable of killing all the propagules and spores of microorganisms (including pathogenic and pathogenic bacteria) in an object is called sterilization. And (3) sterilization: the method or action capable of killing pathogenic bacteria is called sterilization, and the medicine with sterilization action is called disinfectant or germicide, and is effective for only breeding bacteria under the common concentration, and has no harmful action for spore. Bacteriostasis: a method or effect that prevents or inhibits the growth of microorganisms is called preservation or bacteriostasis. Drugs used for preservation are called preservatives or bacteriostats. Many drugs only have bacteriostatic action at low concentration, and can have bactericidal action when the concentration is increased or the action time is long, and the bactericidal action and the bacteriostatic action are generally called as antibacterial action.
The developed antibacterial ABS mainly has the function of inhibiting microorganisms by adding chemical agents (antibacterial agents). While in general, higher concentrations of chemical agents can kill bacteria, lower concentrations can sometimes only kill bacteria, or can otherwise stimulate bacterial growth. The content of the antibacterial agent in the antibacterial ABS is limited, and the antibacterial performance of the antibacterial ABS is determined by the content of the antibacterial agent.
Generally, the antibacterial property of the antibacterial ABS is detected by microbiology, bacterial bead culture is carried out in advance, ABS plastic particles are pressed into a flat sheet-shaped plate with the thickness of 5 cm multiplied by 0.5 cm through secondary processing, the cultured bacterial beads are inoculated on the plate, the microbiological culture is carried out again, and the size of a bacteriostatic circle of the sheet is detected to analyze the antibacterial property of the ABS. The microbiological detection is suitable for detecting the antibacterial activity of the antibacterial ABS finished product, the detection result is visual and convincing, but the microbiological detection is applied to guiding the adjustment of the process parameters in the production process of the antibacterial ABS body, and the requirement of continuous production of the antibacterial ABS product is limited to a certain extent because the microbiological detection cannot be used for quickly detecting the antibacterial performance of the product due to the long period.
Disclosure of Invention
(I) technical problems to be solved by the invention
The invention aims to solve the technical problem that microbiological detection on the antibacterial activity period of an antibacterial ABS product is long and cannot be used for rapidly guiding the adjustment of the addition ratio of an antibacterial agent in the process of producing the antibacterial ABS product by a bulk method, and provides a novel method for detecting the antibacterial effect of the ABS product.
(II) the technical scheme adopted by the invention
The method of the invention is under the specific process, make the corresponding relation of the target metal content in the antibacterial ABS and the antibacterial property of the product into the standard curve, in the actual production application, only need to detect the content of the target metal in the antibacterial ABS product, look for the above-mentioned standard curve, can judge the antibacterial effect of the antibacterial ABS product fast and accurately, has greatly shortened the detection cycle of ABS antibacterial property, has reduced the detection cost, has raised the detection efficiency, more importantly, has offered the feasibility monitoring means for using the method of the body process to produce antibacterial ABS, have solved because of the little birth to name the detection method detects ABS antibacterial effect cycle long, can't be used for guiding the difficult problem of the production of antibacterial ABS of the body process.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the invention sets the metal contained in the antibacterial agent as the target metal. Firstly, establishing a harrowing metal content-antibacterial effect standard curve according to a method for detecting the antibacterial effect of antibacterial ABS in microbiology and by combining a harrowing metal measuring method used in the invention; secondly, after the antibacterial ABS is subjected to ashing, dissolving, acidifying, constant volume, interference prevention and other treatments, the concentration of the target metal in the sample to be detected is measured by an analytical instrument; and finally, according to the content of the harrowing metal in the sample to be detected, searching the position of the harrowing metal in a harrowing metal content-antibacterial effect standard curve, comparing the effective antibacterial content in the standard curve, and judging the antibacterial performance of the antibacterial ABS.
A method for rapidly detecting antibacterial performance of an antibacterial ABS product in production comprises the following steps:
the method comprises the following steps: establishing a target metal content-antibacterial effect standard curve;
1.1 preparing two identical batches of a series of antibacterial ABS containing target metals in different proportions;
1.2 according to standard detection methods of QB/T2591-2003 and GB4789.2-2016, a batch of antibacterial ABS containing different proportions of targeted metals is subjected to microbiological antibacterial activity detection to obtain the antibacterial rate of a series of antibacterial ABS containing different proportions of targeted metals;
1.3, respectively placing another batch of antibacterial ABS containing target metals in different proportions in a quartz crucible, after full ashing, dissolving ash substances cooled to room temperature with acid solution, alkali solution or water, drying, dissolving with a volumetric flask to a constant volume, taking out the solution from the volumetric flask, measuring the concentration of the target metal ions in the solution, and calculating the content of the target metals in the antibacterial ABS;
1.4 establishing a target metal content-antibacterial effect standard curve by using the antibacterial rate in the step 1.2 and the content of the target metal in the antibacterial ABS obtained in the step 1.3;
step two: detecting the content of the target metal in the antibacterial ABS sample;
calculating the content of the targeted metal in the antibacterial ABS containing the targeted metal according to the process in the step 1.3;
step three: and (4) according to the content of the target metal obtained by calculation in the step two, judging the antibacterial performance of the antibacterial ABS sample containing the target metal by utilizing the content of the target metal-the antibacterial effect standard curve.
Furthermore, the target metal in the antibacterial agent is silver, zinc, cadmium or copper, and the metal element in the antibacterial agent exists in the antibacterial agent in the form of atoms, ions or complexes. The metal elements in the antibacterial agent can be used as target targets in content detection.
Furthermore, the content range of the targeted metal antibacterial agent in the antibacterial ABS is 0.1-10%.
Further, in the first step, the acid solution used for dissolving, acidifying, diluting and fixing the volume of the ash substance is one or more of concentrated nitric acid, concentrated perchloric acid, concentrated sulfuric acid and concentrated hydrochloric acid; the alkali solution is sodium hydroxide aqueous solution or potassium hydroxide aqueous solution; the water is deionized water or purified water.
Further, in the first step, the method for determining the concentration of the targeted metal ions in the solution comprises Atomic Absorption Spectrometry (AAS), ultraviolet-visible spectrophotometry (UV), Atomic Fluorescence (AFS), electrochemical-anodic stripping voltammetry, X-ray fluorescence spectrometry (XRF), inductively coupled plasma mass spectrometry (ICP-MS), and other methods which can be used for quantitatively detecting the concentration of heavy metal elements in the filtrate after the treatment.
Further, in the first step, a calculation formula for the content of the target metal in the antibacterial ABS is calculated:
Figure BDA0002737370460000041
content of C-targeting metal in the antibacterial ABS,% (mass fraction);
c1-the concentration of target metal, w/v (mass to volume ratio), detected by an analytical instrument in a sample;
v-sample size, V, (volume unit);
x-total dilution factor;
w-total ashed sample, g, (mass units).
Furthermore, in the first step, the dosage range of the quantitative ABS plastic particles is 1-100 g.
Technical effects
1. The problems that the antimicrobial ABS has long antimicrobial effect period and cannot be used for guiding the production of the body process in time due to microbiological detection can be solved;
2. a feasible monitoring means is provided for producing the antibacterial ABS by using a bulk process method;
3. the antibacterial effect of the antibacterial ABS product can be rapidly and accurately judged, the detection period of the antibacterial property of the ABS is greatly shortened, the detection cost is reduced, and the detection efficiency, the qualification rate of the product, the continuous operation period and the yield are improved.
Drawings
FIG. 1 is a standard curve of the content of target metal (silver) -antibacterial effect in example 1;
fig. 2 is a standard curve of the content of the target metal (silver) -antibacterial effect in example 3.
Detailed Description
Example 1
The ABS antibacterial performance of an antibacterial body produced by a certain process by taking a nano-silver antibacterial agent as an antibacterial raw material is detected.
The method comprises the following steps: establishing a standard curve of the content of the target metal (silver) -the antibacterial effect
Certain nano silver is used as an antibacterial agent, different proportions are respectively added, and the antibacterial ABS with different antibacterial agent contents is processed by adopting an antibacterial ABS processing technology or an equivalent technology.
Performing microbiological antibacterial activity detection on the antibacterial ABS according to standard detection methods of QB/T2591-2003 and GB4789.2-2016, wherein the antibacterial ABS has an antibacterial rate of more than or equal to 99 percent and is defined as having good antibacterial property; the antibacterial rate is more than or equal to 90 percent and less than 99 percent, and the antibacterial property is defined; an antibacterial rate of < 90% is defined as no antibacterial activity. A record is made (in particular the sample numbers at the antimicrobial activity nodes are marked).
Weighing 10 g of each antibacterial ABS sample, accurately measuring to 0.001 g, placing the samples in a quartz crucible, ashing for 5 hours at 450 ℃, cooling, dissolving and soaking for 30 minutes by using 10 ml of a mixed solution of 0.1N nitric acid and 0.1N perchloric acid (nitric acid: perchloric acid is 9: 1 in volume ratio), drying the mixed solution in the crucible to about 2 ml at 110 ℃, cooling to room temperature, cleaning all residual liquid in the crucible to a volumetric flask of 1000 ml by using 10-50 ml of 0.01N nitric acid, diluting to scale by using water, and detecting the content of the targeted metal silver by using a graphite furnace atomic absorption spectrometer.
The node content in the target metal antibacterial content curve is respectively represented by a1 and a 2; b1, b 2; c1, c2, c 3.
And (3) adopting graphite furnace atomic absorption spectroscopy, selecting a cathode hollow lamp with the wavelength of 328.1nm for irradiation, measuring the concentration of silver ions in each sample treated by the method, and calculating to obtain the following silver content values:
a1=0.00164%,a2=0.00203%;
b1=0.00185%,b2=0.00387%
c1=0.00296%,c2=0.00408%,c3=0.00549%
according to the antimicrobial activity detection data and the silver content detection data of the microorganisms, an antimicrobial activity curve is drawn as shown in the following figure 1.
Step two, detecting the content of the target metal in the sample
The antimicrobial addition ratios were 0.1%, 0.15%, 0.2%, 0.3% for the bulk ABS sample 1, sample 2, sample 3, and sample 4 produced, respectively. Weighing 10 g of the 4 samples, accurately weighing the samples to 0.001 g, correspondingly placing the samples in 4 quartz crucibles with numbers 1#, 2#, 3# and 4#, moving the quartz crucibles to a high-temperature furnace at 450 ℃ for ashing for 5 hours, dissolving and soaking ash in the 4 quartz crucibles by using 10 ml of mixed solution of 0.1N nitric acid and 0.1N perchloric acid (nitric acid: perchloric acid is 9: 1 in volume ratio) for 30 minutes, drying the solutions in the 4 crucibles to about 2 ml (fully performing acidolysis) at 110 ℃, cooling to room temperature, completely cleaning the substances in the crucibles by using 10 to 50 ml of 0.1N nitric acid, transferring the substances to 1000 ml volumetric flasks with numbers 1#, 2#, 3# and 4# respectively, and diluting the substances to the scale by using water for standby.
And (3) adopting graphite furnace atomic absorption spectroscopy, selecting a cathode hollow lamp with the wavelength of 328.1nm for irradiation, determining the concentration of silver ions in the four processed samples, and calculating to obtain the silver contents of 0.00217%, 0.00329%, 0.00437% and 0.00672% in the four antibacterial ABS samples.
And step three, searching the position of the targeted metal content in the sample in the targeted metal antibacterial concentration curve, and judging the antibacterial effect of the sample.
The positions of the targeted metal contents in the sample in the targeted metal antibacterial concentration curve are as follows:
sample 1: 0.00217% > a 2; b1 < 0.00217% < b 2; 0.00217% < c 1;
sample 2: 0.00329% > a2, b1 < 0.00329% < b 2; c1 < 0.00329% < c 2;
sample 3: 0.00437% > a2, 0.00437% > b2, c2 < 0.00437% < c 3;
sample 4: 0.00672% > a2, 0.00672% > b2, 0.00672% > c 3.
The antibacterial effect is judged according to the content of the target metal in the sample:
the sample 1 has good escherichia coli resistance, can resist candida albicans, and has no mould prevention effect;
the sample 2 has good escherichia coli resistance, can resist candida albicans and can achieve a level II mildew-proof effect;
sample 3 has good resistance to escherichia coli and candida albicans, and can achieve the level I mildew-proof effect;
sample 4 has good resistance to escherichia coli and candida albicans, and can achieve a level 0 mildew-proof effect.
The four samples are tested and verified for antibacterial activity by a microbiological detection method, and the result is as follows: the antibacterial rate of Escherichia coli of the sample 1 is more than 99 percent, the antibacterial rate of Candida albicans is more than 90 percent and less than 99 percent, and the mould is not prevented; the antibacterial rate of Escherichia coli of the sample 2 is more than 99 percent, and the antibacterial rate of Candida albicans is more than 90 percent and less than 99 percent; the antibacterial rate of the mould reaches the level II effect; sample 3, the antibacterial rate of escherichia coli is more than 99%; the antibacterial rate of the candida albicans is more than 99 percent; the antibacterial rate of the mould reaches the I level effect; sample 4 Escherichia coli antibacterial rate > 99%; the antibacterial rate of the candida albicans is more than 99 percent; the antibacterial rate of the mould reaches 0 grade effect. The results were consistent with the test results of the present invention.
Example 2
The results of the microbiological detection method for the antimicrobial activity test of the antimicrobial bulk ABS produced by using the nano-silver antimicrobial agent in example 1 as the antimicrobial raw material and adding different proportions through a certain process are as follows: sample 5, the antibacterial rate is more than 99%, and the mould-proof effect of grade I is achieved, and sample 6, the antibacterial rate is less than 60%, and the mould-proof effect is not achieved.
Weighing 10 g of two samples, accurately measuring the two samples to 0.001 g, respectively placing the two samples into 2 quartz crucibles with numbers 5# and 6# respectively, moving the two samples to a high-temperature furnace at 450 ℃ for ashing for 5 hours, respectively dissolving and soaking ash in the 2 quartz crucibles by using 10 ml of mixed solution of 0.1N nitric acid and 0.1N perchloric acid (nitric acid: perchloric acid is 9: 1) for 30 minutes, respectively drying the solution in the 2 crucibles to about 2 ml (fully acidolyzing) at 110 ℃, cooling the solution to room temperature, completely cleaning the substances in the crucibles by using 10 ml to 50 ml of 0.01N nitric acid, respectively transferring the substances to 2 1000 ml volumetric flasks with numbers 5# and 6# respectively, and diluting the substances to the scale by using water for standby.
And detecting the silver content in the two samples by using graphite furnace atomic absorption spectroscopy.
Sample 5 is 0.00474%, is greater than a2, is greater than b2, is between c2 and c3, has the performance of resisting escherichia coli and candida albicans, and has grade I mildew-proof effect.
Sample 6 was 0.00108%, less than a1, less than b1, less than c 1. No antibacterial property and no mould resistance.
The silver content detection judgment results of the samples 5 and 6 are consistent with the microbiological detection results.
Example 3
Detection of antibacterial property of antibacterial ABS (acrylonitrile butadiene styrene) body produced by using antibacterial material containing zinc ions through certain process
Step one, establishing a targeted metal (zinc) content-antibacterial effect standard curve
Certain zinc ion-containing antibacterial material is used as an antibacterial agent, different proportions are respectively added, and the antibacterial ABS with different antibacterial agent contents is processed by adopting an antibacterial ABS processing technology or an equivalent technology. The microbiological antibacterial activity of each antibacterial ABS was tested and recorded according to the standard test methods of QB/T2591-2003 and GB4789.2 (especially, the sample numbers at the antibacterial activity nodes are marked).
Weighing 30 g of each antibacterial ABS sample, accurately weighing the samples to 0.001 g, placing the samples in a quartz crucible, ashing for 5 hours at 400 ℃, cooling, dissolving and soaking for 30 minutes by using 10 ml of a mixed solution of 0.1N nitric acid and 0.1N perchloric acid (nitric acid: perchloric acid is 9: 1 in volume ratio), drying the mixed solution in the crucible to about 2 ml at 110 ℃, cooling to room temperature, washing all residual liquid in the crucible to a volumetric flask of 500 ml by using 10 to 50 ml of 0.01N nitric acid, and diluting to a scale with water for later use.
The node concentrations in the target metal antibacterial concentration curve are respectively u1 and u 2; v1, v 2; w1, w2 and w 3.
And (2) detecting the zinc concentration of each sample to be detected by adopting a flame atomic absorption spectrometer and a zinc cathode hollow lamp under the wavelength of 213.9nm, and calculating to obtain the following zinc content numerical values:
u1=0.00483%,u2=0.00629%;
v1=0.00657%,v2=0.00951%;
w1=0.00733%,w2=0.01243%,w3=0.01606%
according to the antimicrobial activity detection data of the microorganisms and the detection data of the concentration of zinc ions, an antimicrobial activity curve is drawn as shown in figure 2.
Step two, detecting the content of the target metal in the sample
The addition ratio of the antibacterial agent is 0.5%, 1%, 1.5% and 2% respectively, 30 g of each antibacterial ABS sample is weighed, the weighed sample is accurately 0.001 g, the weighed sample is placed in quartz crucibles numbered as 7#, 8#, 9# and 10#, the quartz crucibles are ashed at 400 ℃ for 5 hours, after cooling, 10 ml of mixed solution of 0.1N nitric acid and 0.1N perchloric acid (nitric acid: perchloric acid is 9: 1 in volume ratio) is used for dissolving and soaking for 30 minutes, then the mixed solution in the crucibles is dried at 110 ℃ to about 2 ml, after cooling to room temperature, 10 ml to 50 ml of 0.01N nitric acid is used for cleaning all residual liquid in the crucibles to 500 ml volumetric flasks numbered as 7#, 8#, 9# and 10# for standby, and the residual liquid is diluted to the scale by water.
The zinc concentration in the four samples is detected by adopting a flame atomic absorption spectrometer and a zinc cathode hollow lamp under the wavelength of 213.9nm, and the zinc content in each antibacterial ABS is calculated to be 0.00204%, 0.00465%, 0.00632% and 0.00827% respectively.
And step three, searching the position of the targeted metal content in the sample in the targeted metal antibacterial concentration curve, and judging the antibacterial effect of the sample.
Sample 7: 0.00204% < u1, 0.00204% < v1, 0.00204% < w 1;
sample 8: 0.00465% < u1, 0.00465% < v1, 0.00465% < w 1;
sample 9: 0.0632 > u2, 0.0632 < v1, 0.0632 < w 1;
sample 10: 0.0827 & gt u2, v1 & lt 0.0827 & lt v2, w1 & lt 0.0827 & lt w2
The measured values of the sample 7 and the sample 8 are less than u1, v1 and w1, and the antibacterial property and the mould-proof effect are not achieved;
sample 9 had good anti-escherichia coli performance, failed to resist candida albicans, and had no anti-fungal effect;
the sample 10 has good escherichia coli resistance, can resist candida albicans and can achieve the level II anti-mould effect.
The antimicrobial activity was measured by microbiological assay, which resulted in: the antibacterial rate of Escherichia coli of a sample 7 is less than 90 percent, the antibacterial rate of Candida albicans is less than 90 percent, and the mould is not prevented; the antibacterial rate of Escherichia coli of a sample 8 is less than 90 percent, and the antibacterial rate of Candida albicans is less than 90 percent; the mould is not prevented; sample 9 has an Escherichia coli antibacterial rate of more than 99%; the antibacterial rate of the candida albicans is less than 90 percent; the mould is not prevented; the antibacterial rate of Escherichia coli of a sample 10 is more than 99 percent; the antibacterial rate of Candida albicans is more than 90% and less than 99%, and the level II mildew-proof effect is achieved. The results were consistent with the test results of the present invention.
Example 4
The antibacterial ABS bulk is produced by an antibacterial material containing zinc ions through a certain process, and the antibacterial activity test result is as follows: sample 11, the antibacterial rate is more than 99%, and the mould proofing of grade I can be achieved; sample 12, with an antibacterial rate > 90%, but not mould proof.
Weighing 30 g of each of the two antibacterial ABS samples, accurately weighing the samples to 0.001 g, placing the samples in quartz crucibles with the numbers of 11# and 12# respectively, ashing the samples for 5 hours at 400 ℃, cooling the samples, dissolving and soaking the samples for 30 minutes by using 10 ml of mixed solution of 0.1N nitric acid and 0.1N perchloric acid (the nitric acid: the perchloric acid is 9: 1 in volume ratio), drying the mixed solution in the crucibles to about 2 ml at 110 ℃, cooling the mixed solution to room temperature, respectively washing all residual liquid in the crucibles by using 10 ml to 50 ml of 0.01N nitric acid to 500 ml volumetric flasks with the numbers of 11# and 12# respectively, and diluting the residual liquid to the scale for later use.
And (2) detecting the zinc concentration of the two samples to be detected by adopting a flame atomic absorption spectrometer and a zinc cathode hollow lamp under the wavelength of 213.9nm, and calculating to obtain the following zinc content numerical values:
sample 11 is 0.01408%, more than u2, more than v2, between w2 and w3, has good performance of resisting escherichia coli and candida albicans, and can achieve I-grade mildew-proof effect;
sample 12 was 0.00609%, between u1 and u2, less than v1, less than w1, with anti-E.coli, not anti-Candida albicans, no anti-mildew effect.
The detection results of the samples 11 and 12 are consistent with the results judged by the microbiological detection method.
Table 1 is a comparison table of the antibacterial effect of ABS determined by the detection of the content of the target metal in examples 1-4 and the antibacterial effect of ABS determined by the microbiological detection method
TABLE 1 comparison of results of targeted metal content testing and microbiological testing
Figure BDA0002737370460000091
Figure BDA0002737370460000101
("+" indicating antibacterial property, "+ +" indicating excellent antibacterial property, "-" indicating no antibacterial property)
As can be seen from the data in the table, the antibacterial performance of ABS judged by the method of detecting the content of the target metal by using an instrument is consistent with the result of microbiological detection. A method for rapidly detecting the antibacterial performance of an antibacterial ABS product in production can replace a microbiological detection method in production, rapidly judge the antibacterial effect of ABS and improve the production efficiency.

Claims (9)

1. A method for rapidly detecting antibacterial performance of an antibacterial ABS product in production is characterized by comprising the following steps:
the method comprises the following steps: establishing a target metal content-antibacterial effect standard curve;
1.1 preparing two identical batches of a series of antibacterial ABS containing target metals in different proportions;
1.2 according to standard detection methods of QB/T2591-2003 and GB4789.2-2016, a batch of antibacterial ABS containing different proportions of targeted metals is subjected to microbiological antibacterial activity detection to obtain the antibacterial rate of a series of antibacterial ABS containing different proportions of targeted metals;
1.3, respectively placing another batch of antibacterial ABS containing target metals in different proportions in a quartz crucible, after full ashing, dissolving ash substances cooled to room temperature with acid solution, alkali solution or water, drying, dissolving with a volumetric flask to a constant volume, taking out the solution from the volumetric flask, measuring the concentration of the target metal ions in the solution, and calculating the content of the target metals in the antibacterial ABS;
1.4 establishing a target metal content-antibacterial effect standard curve by using the antibacterial rate in the step 1.2 and the content of the target metal in the antibacterial ABS obtained in the step 1.3;
step two: detecting the content of the target metal in the antibacterial ABS sample;
calculating the content of the targeted metal in the antibacterial ABS containing the targeted metal according to the process in the step 1.3;
step three: and (4) according to the content of the target metal obtained by calculation in the step two, judging the antibacterial performance of the antibacterial ABS sample containing the target metal by utilizing the content of the target metal-an antibacterial effect standard curve.
2. The method for rapidly detecting the antibacterial performance of the antibacterial ABS product in production according to claim 1, wherein the target metal in the antibacterial agent is silver, zinc, cadmium or copper.
3. The method for rapidly detecting the antibacterial performance of the antibacterial ABS product in production according to claim 2, wherein the metal element in the antibacterial agent exists in the antibacterial agent in the form of atom, ion or complex.
4. The method for rapidly detecting the antibacterial performance of the antibacterial ABS product in production according to claim 1, wherein the content range of the targeted metal antibacterial agent in the antibacterial ABS is 0.1-10%.
5. The method for rapidly detecting the antibacterial performance of the antibacterial ABS product in production according to claim 1, wherein in the first step, the ashing temperature is 300-900 ℃.
6. The method for rapidly detecting the antibacterial performance of the antibacterial ABS product in production according to claim 1, wherein in the first step, the acid solution used for dissolving, acidifying, diluting and diluting the ash substance to a constant volume is one or more of concentrated nitric acid, concentrated perchloric acid, concentrated sulfuric acid and concentrated hydrochloric acid; the alkali solution is sodium hydroxide aqueous solution or potassium hydroxide aqueous solution; the water is deionized water or purified water.
7. The method for rapidly detecting the antibacterial performance of the antibacterial ABS product in production according to claim 1, wherein in the first step, the method for determining the concentration of the target metal ions in the solution comprises atomic absorption spectrometry, ultraviolet-visible spectrophotometry, atomic fluorescence, electrochemistry-anodic stripping voltammetry, X-ray fluorescence spectrometry and inductively coupled plasma mass spectrometry.
8. The method for rapidly detecting the antibacterial performance of the antibacterial ABS product in production according to claim 1, wherein in the first step, the formula for calculating the content of the target metal in the antibacterial ABS is as follows:
Figure FDA0002737370450000021
wherein: content of C-targeting metal in the antibacterial ABS,% (mass fraction);
c1-the concentration of target metal, w/v (mass to volume ratio), detected by an analytical instrument in a sample;
v-sample size, V, (volume unit);
x-total dilution factor;
w-total ashed sample, g, (mass units).
9. The method for rapidly detecting the antibacterial performance of the antibacterial ABS product in production according to claim 1, wherein the dosage range of the quantitative ABS plastic granules is 1-100 g.
CN202011138191.XA 2020-10-22 2020-10-22 Method for rapidly detecting antibacterial performance of antibacterial ABS product in production Pending CN112198130A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008209347A (en) * 2007-02-28 2008-09-11 Mitsubishi Heavy Ind Ltd Antimicrobial performance evaluating method
CN101805780A (en) * 2010-03-18 2010-08-18 曲阜师范大学 Quantitative determination method of antibacterial property of titanium dioxide nanotube
CN103728394A (en) * 2014-01-15 2014-04-16 中华人民共和国苏州出入境检验检疫局 Daily chemical product antibacterial agent detection method based on graphene oxide solid phase extraction
CN106124432A (en) * 2016-06-22 2016-11-16 齐齐哈尔大学 A kind of method of rational judgment material antibiotic rate and application thereof
CN107607512A (en) * 2017-10-22 2018-01-19 贺州学院 A kind of method of content of beary metal in AFS measure edible mushroom
CN109187609A (en) * 2018-09-05 2019-01-11 科立视材料科技有限公司 A kind of anti-microbial effectiveness evaluation method of antibiotic glass
CN110272958A (en) * 2019-03-15 2019-09-24 秦皇岛出入境检验检疫局检验检疫技术中心 ATP bioluminescence lgCA-lgIAThe method of calibration curve method detection antibiotic paint fungicidal properties
CN110527707A (en) * 2019-10-14 2019-12-03 北京大学第一医院 A kind of detection method of material surface anti-microbial property

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008209347A (en) * 2007-02-28 2008-09-11 Mitsubishi Heavy Ind Ltd Antimicrobial performance evaluating method
CN101805780A (en) * 2010-03-18 2010-08-18 曲阜师范大学 Quantitative determination method of antibacterial property of titanium dioxide nanotube
CN103728394A (en) * 2014-01-15 2014-04-16 中华人民共和国苏州出入境检验检疫局 Daily chemical product antibacterial agent detection method based on graphene oxide solid phase extraction
CN106124432A (en) * 2016-06-22 2016-11-16 齐齐哈尔大学 A kind of method of rational judgment material antibiotic rate and application thereof
CN107607512A (en) * 2017-10-22 2018-01-19 贺州学院 A kind of method of content of beary metal in AFS measure edible mushroom
CN109187609A (en) * 2018-09-05 2019-01-11 科立视材料科技有限公司 A kind of anti-microbial effectiveness evaluation method of antibiotic glass
CN110272958A (en) * 2019-03-15 2019-09-24 秦皇岛出入境检验检疫局检验检疫技术中心 ATP bioluminescence lgCA-lgIAThe method of calibration curve method detection antibiotic paint fungicidal properties
CN110527707A (en) * 2019-10-14 2019-12-03 北京大学第一医院 A kind of detection method of material surface anti-microbial property

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